Solid State Synthesis of Mixed Metal Oxides

Tornés-Blanco AnibalAlicea-Pauneto AbneilColón-Rivera RamónGonzález-Piñeiro Ann

INTRODUCTION

Background Info

❏ Solid-state synthesis ❏ Branch of material chemistry : Mix &

match solids.❏ Why is this study so important?

❏ Obtain new compounds with unique properties to aid the technologically dependent world we live in.

Cornerstone of technology

❏ Superconductors such as high purity silicon and catalysts like platinum,

took a pivotal role in the industrialization process during the 20th century.

Chen et al. 2015

“In recent years, electrochemical capacitors, also known as supercapacitors, have received a large amount of attention as an important power storage device due to their high power density, fast recharge capability and long cycle life .”

Related Works

Koscielski et al. 2012

Problem

❏ Synthesize new compounds from the combination of different metals from the families 13, 14, 15, chalcogens (group 16) and intrinsic Oxygen.

Hypothesis❏ After heat application, oxidation reactions will occur and

hopefully, crystals will appear .

❏ This is a trial and error experimentation

METHODOLOGY

Reactions

Ternary Quaternary

1 In : 1 Sb 1 S : 1 Bi : 1 In

1 In : 1 Bi 1 Pb : 1 Sn : 1 S

2 In : 1 Sn 2 In : 1 Sn : 1S

2 In : 1 Pb 2 In : 1 Sn : 2 S

Ternary Quaternary

5 In : 3 Sb 1 Co : 2 In : 1 S

5 Sn : 3 Pb 1 Co : 1 Bi : 1 S

5 Bi : 3 Pb 1 In : 2 Co : 2 S

1 Bi : 2 Pb 1 In : 1 Bi : 1 S

Methodology

Element Selection & Weighing

Carbon CoatingSilica Tube Split

http://chemistry.stackexchange.com/questions/18968/why-does-a-glass-tube-show-white-bands-after-being-heated-with-a-torch

http://instrumentosdelaboratorio.org/balanza-de-laboratorio

http://oxypetrol.com/ https://www.flickr

.com/photos/fallenangel8/2503298659/

Methodology

Transfer the reaction to the tube

Heat in the GSL-1100x “Lisa”

”

Results Analysisvia Microscope

http://instrumentosdelaboratorio.org/espatula-de-laboratorio

Heating Curve

Cooling

Heating

Liquid/Solid

Results

We found Crystals!

But not the type we expected...

Ternary Reactions I 5 In : 3 Sb 5 Sn : 3 Pb

Ternary Reactions II 5 Bi : 3 Pb 1 Bi : 2 Pb

Ternary Reactions III1 In : 1 Sb 1 In : 1 Bi

Ternary Reactions IV 2 In : 1 Sn 2 In : 1 Pb

Conclusions

❏ The results were partially positive making allusions to our

hypothesis.

❏ We obtained Oxide Powder.

Limitations

❏ Time Limitation

❏ Only one high temperature vacuum tube furnace,

named ¨Lisa¨ .

❏ Oxygen insulating equipment

Future Work

❏ Try new combinations of ternary and quaternary

compounds

❏ Analyze the data collected with the appropriate

instrumentation

ReferencesChen S, Xue M, Li Y, Zhu L, Zhang D, Fang Q, Qiu S. 2015. Porous ZnCo2O4

nanoparticles derived from a new mixed-metal organic framework for supercapacitors. Royal Society of Chemistry (RSC) (2) . [2014 Oct 17, cited 2015 April 29] 2:(177-183). DOI: 10.1039/c4qi00167b

C. Z. Yuan, L. Yang, L. R. Hou, L. F. Shen, X. G. Zhang and X. W. Lou, Energy Environ. Sci., 2012, 5, 7883.

Koscielski L, Ringe E, Van Duyne R, Ellis D, Ibers J. 2012. Single-Crystal Structures, Optical Absorptions, and Electronic Distributions of Thorium Oxychalcogenides ThOQ (Q= S, Se, Te). American Chemical Society dx.doi.org/10.1021/ic300510x | Inorg. Chem. 2012, 51, 8112−8118.

Acknowledgements

● RISE Program at UPR Cayey

● Omar Padilla

● Christopher Bernard

● Andres Diaz

● Maria Rivera

● Roberto González

In Memory of Dr. Lukasz A. Koscielski